HuagongsheHuagongshe Chemistry Print Report · For research reference only
Tetrahydrofuran → HCID 23445108, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Tetrahydrofuran | HCID 8028 | — |
| Reactant | Potassium Sodium Tartrate | HCID 9357 | — |
| Reactant | 1-(3,4-dichloro-phenyl)-5-methyl-1H-imidazole-4-carboxylic acid ethyl ester | HCID 69042749 | — |
| Product | HCID 23445108 | HCID 23445108 | — |
Reaction Steps
To a solution of 1-(3,4-dichloro-phenyl)-5-methyl-1H-imidazole-4-carboxylic acid ethyl ester (0.82 g, 2.7 mmol) in THF (27 ml) lithium aluminum hydride (0.21 g, 5.4 mmol) was added portionwise keeping T<10° C. The mixture was stirred in an ice-bath for 2 h, then 1 ml saturated aqueous Seignette salt solution was slowly added. After dilution with AcOEt (100 ml) the mixture was filtered, concentrated and chromatographed [silica, elution with gradient CH2Cl2 to 80% (CH2Cl2/MeOH=9:1)]. The title compound was obtained as a white crystalline solid (0.46 g, 66%). Mp. 174-175° C. (CH2Cl2/iPr2O), MS: m/e=256 (M+)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06667335B2 |
| Source dataset | uspto-grants-2003_12 |
| ORD ID | ord-fd0c8ce8b9a9463b864185e0e396d96d |
| Source note | uspto-grants-2003_12 |